Method for preparation of an alane-etherate complex and alane
View Patent ↗The invention relates to methods of forming an alane-etherate complex and α-alane from the alane-etherate complex. The methods include reacting an alkyl halide with a metal alanate in a solvent including an ether. A tertiary amine may also be added to the reaction. The alane is collected after removal of the solvent and/or the tertiary amine. An electrospraying process can be used to remove the solvent.
1. A method of producing solid α-alane comprising:
reacting one or more alkyl halides with one or more metal alanates in a solvent comprising an ether to form an alane-ether mixture;
removing the solvent from the alane-ether mixture by spray desolvation;
annealing the spray desolvated alane; and,
collecting the solid α-alane;
wherein the solid α-alane exhibits a range of particle sizes of either a range of from 1 μm to 500 nm or a range of from 300 nm to 100 nm.
2. The method of claim 1 , wherein a single alkyl halide is used.
3. The method of claim 1 , wherein a single metal alanate is used.
4. The method of claim 1 , wherein the alkyl halide comprises one of benzyl chloride and n-butyl bromide.
5. The method of claim 1 , wherein the alkyl metal halide comprises n-butyl bromide.
6. The method of claim 1 , wherein the metal alanate comprises sodium aluminum hydride.
7. The method of claim 1 , wherein the solvent comprises diethyl ether.
8. The method of claim 1 , wherein the method includes adding a tertiary amine in the step of forming the alane-etherate mixture.
9. The method of claim 8 , wherein the tertiary amine is removed.
10. The method of claim 8 , wherein the tertiary amine comprises a trialklylamine.
11. The method of claim 1 , wherein the metal alanate comprises lithium aluminum hydride.
12. A method of producing α-alane comprising:
reacting one or more alkyl halides with sodium aluminum hydride in a solvent comprising toluene, ether, a trialkylamine, and a metal halide to form an alane solution;
removing the trialkylamine by sparging the alane solution with an inert gas;
removing the metal halide from the alane solution;
removing ether from the alane solution by distillation; and,
collecting the solid α-alane.
13. The method of claim 12 , wherein removing ether from the alane solution comprises vacuum distillation.
14. The method of claim 1 , wherein the spray desolvation comprises electrospinning the alane-ether mixture.
15. The method of claim 1 , wherein the spray desolvation comprises electrospraying the alane-ether mixture.
16. The method of claim 15 , wherein the annealing comprises heating at a temperature from greater than 60° C. to less than 120° C.
17. The method of claim 16 , wherein the temperature is at least 65° C.
18. The method of claim 16 , wherein the temperature is no greater than 100° C.
19. The method of claim 16 , wherein the annealing is done at a temperature of from 65° C. to 100° C.
20. The method of claim 6 , wherein the solvent further comprises a soluble Li + species.
21. The method of claim 12 , wherein the solvent comprises toluene and diethyl ether, and the ether is removed by distilling the ether from the alane solution until the alane solution contains 8% to 10% ether.